An effective method was developed for the determination of 16 polycyclic aromatic hydrocarbons(PAHs) in Alpinia oxyphylla Miq based on gas chromatography-mass spectrometry(GC-MS).The samples were separated on a DB-EUPAH capillary chromatography column,detected by GC-MS with electron ionization source in selective ion mode,and quantified by stable isotope internal standard method.The optimal extraction conditions were as follows:2.0 g of sample was added with isotope standard solution,then mixed with absolute ethanol and water to dissolve,followed by addition of 10 mL n-hexane for extraction.The extract was firstly subjected to solid-phase extraction with a Florisil column,then saponified with KOH-ethanol solution,and extracted again by solid-phase extraction with a polycyclic aromatic hydrocarbon molecularly imprinted column,finally,eluted with 5 mL dichloromethane-n-hexane(1∶1,by volume).Results showed that the 16 PAHs presented good linear relationships in the concentration range of 1.0-200.0 μg/L with correlation coefficients(r2) not less than 0.992 5.The limits of detection were in the range of 0.3-1.0 μg/kg,and the limits of quantitation were 1.0-3.0 μg/kg.The average recoveries(n=6) for benzo[c] fluorene(BcFL) ranged from 65.4% to 72.8%,with intra-day relative standard deviations(RSD,n=6) of 6.0%-7.4% and inter-day relative standard deviations(RSD,n=6) of 8.5%,respectively,while the average recoveries for the other 15 PAHs were in the range of 89.3%-116%,with intra-day RSDs(n=6) of 0.10%-6.1% and inter-day RSDs(n=6) of 1.2%-7.5%,respectively.The developed method showed excellent purification effect,sensitivity and high accuracy,and was suitable for the simultaneous determination of 16 PAHs in Alpinia oxyphylla Miq.
关键词
气相色谱-质谱法(GC-MS)稳定同位素内标法益智药材多环芳烃(PAHs)基质效应
Keywords
gas chromatography-mass spectrometry(GC-MS)stable isotope internal standard methodAlpinia oxyphylla Miqpolycyclic aromatic hydrocarbon(PAHs)matrix effect
Determination of Perchlorate in Tea by Ultra-high Performance Liquid Chromatography-High Resolution Mass Spectrometry Coupled with Dispersive Micro Solid-phase Extraction
Determination of Quinoline and Isoquinoline in Textiles by Gas Chromatography-Mass Spectrometry
Analysis of Organochlorine Pesticides in Soil by GC-MS with Solid Phase Extraction and Their Matrix Effects Study
Determination of Nano Silver Particles in Environmental Matrix Water by Single Particle Inductively Coupled Plasma Mass Spectrometry
Matrix Effect in Direct Analysis of Raw Solid and Viscous Drugs by Solid-substrate Electrospray Ionization Mass Spectrometry